CoFe 2 O 4 /SiO 2 nanocomposites have been prepared by a sol-gel procedure, starting from tetraethylorthosilicate and metallic nitrates. The formation mechanism of the composites was characterized by differential scanning calorimetry, infrared spectroscopy, transmission electron microscopy, X-ray diffraction and Raman spectroscopy. The magnetic properties were measured using a vibrating sample magnetometer. It was found that xerogel obtained at low temperatures was amorphous. Heat treatment at 400℃ resulted in the partial formation of CoFe 2 O 4 clusters. On further increasing the annealing temperature to 800℃, CoFe 2 O 4 nanocrystals with diameters of ~17 nm could be dispersed in the silica matrix. The formation of CoFe 2 O 4 clusters was accompanied with the rearrangement of silica network, and the enhancement of the interaction between the metal ions and the surrounding silica network. The interaction between the particles and the matrix would be weakened or even disappear when annealing temperature was raised to as high as 800℃. Both the coercive field and the density of magnetization of composites would increase with an increase in the annealing temperature.Recent years see an increasing interest in nanocomposites synthesized by a sol-gel procedure consisting of magnetic nanosized particles embedded in a silica matrix. due to their specific physical and chemical properties [1][2][3][4] . Sol-gel derived amorphous silica matrix is an excellent host for supporting different types of guest nanoparticles. The porous nature of the amorphous silica matrix provides nanomagnetic particles with nucleation sites, and minimizes the aggregation phenomena, imposing an upper limit to the size of the particles [5,6] . However, to the best of our knowledge, this method was mostly used for obtaining nanocomposites that contain oxide of single metal. It was seldom used to prepare the nanocomposites with multi-component metal oxides nanoparticles dispersed in a SiO 2 matrix, which can form a promising class of materials with many new properties. Spinel ferrite nanoparticles, an important multi-component metal oxide, have been intensively investigated in recent years. Our research group has successfully synthesized NiFe 2 O 4 /SiO 2 nanocomposites by a sol-gel technique, and the discussed the effects of various parameters on the particle size [7] .CoFe 2 O 4 is a well-known hard magnetic material with very high cubic magnetocrystalline anisotropy, high coercivity, and moderate saturation magnetization. These properties make it a promising material for high-density magnetic recording [8,9] . In this paper, we report the dispersion of CoFe 2 O 4 nanoparticles in a silica matrix prepared by a sol-gel procedure. The formation mechanism of the nanocomposites was studied by differential scanning calorimetry, IR spectroscopy, Raman spectroscopy, transmission electron micrographs and X-ray diffraction. The magnetic properties were measured using a vibrating sample magnetometer. 1 Experimental Analytical grade tetraethylorthosilicate (T...